CN114395915B - Polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber and preparation method thereof - Google Patents
Polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of new material preparation, and particularly discloses a preparation method of polypropylene hydrocarbon/reduced graphene oxide coaxial coated high-conductivity fibers, which comprises the following steps: (1) preparing an aqueous GO solution; (2) Placing the cleaned waste non-woven polypropylene fabric into a mixed solution of a swelling agent and a surfactant for treatment for a period of time, and then drying to obtain modified non-woven polypropylene fabrics (T-NPFs); (3) Placing the T-NPFs into the GO aqueous solution for infiltration, and then drying to obtain polypropylene hydrocarbon/graphene oxide coaxial coated fibers (GO-NPFs); (4) And (3) placing the GO-NPFs in a reducing agent for treatment, and then cleaning and drying to obtain the polypropylene hydrocarbon/graphene oxide coaxial coated high-conductivity fiber (rGO-NPFs). The method can recycle the W-NPFs, maintain the loose fiber network characteristic of the W-NPFs, and simultaneously endow the NPFs with a functional layer coaxially coated by rGO to provide higher conductivity.
Description
Technical Field
The invention belongs to the technical field of new material preparation, and particularly relates to a polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber and a preparation method thereof.
Background
Nonwoven Polypropylene Fabrics (NPFs) have attracted public attention as air filters for Personal Protection Equipment (PPE) due to the recent global CoVid-19 pandemic, which has led to their mass production to cope with demand. However, the good properties of waste nonwoven polypropylene fabrics (W-NPFs) and white staining after PPE use still cause undeniable dilemma and concern. Some properties of W-NPFs remain after use, where the soft and extremely high specific surface area show a surprising possibility to develop wearable devices, such as flexible energy storage materials, nano-generators, electromagnetic interference shielding, strain sensors and biosensors. All these applications require good electrical conductivity, which is not consistent with the original Properties of Polypropylene (PP). Graphene and its derivatives are therefore incorporated into PP composite systems due to their large surface area to volume ratio, conductivity and chemical activity in two-choice fashion. In particular to reduced graphene oxide (rGO), which plays an important role in synthesis due to the abundant oxygen-containing functional groups of the precursor Graphene Oxide (GO) and the self-controllable conductivity of the reduced graphene oxide (rGO).
Many precursors have passed through respective processes to achieve conductivity, which are largely divided into three categories, in-situ copolymerization, melt blending, and post-formation coating. In situ copolymerization does improve mechanical strength and crystallization behavior, but requires inefficient rGO doping to reach the permeation threshold for target conductivity. Melt blending is similar to in situ copolymerization, and is based on the flowability of PP as a thermoplastic material in the molten state and the shear stress of external equipment on the melt to disperse the filler, depending on the fine choice of dispersant and the complex design of mixing facilities. Both of the above methods require a three-dimensional conductive network of rGO that is either completely dispersed between the polymer chains or locally aggregated along the crystal particle contact surface. The coating is realized by the interaction of the purposely designed outer surface, which is more capable of maintaining the performance of the PP, while part of the interaction may lead to degradation of the PP or disappearance within a few hours. This approach can be inversely divided into sandwich and coaxial cladding structures. The sandwich structure uses NPFs as templates to coat rGO films on the upper and lower sides to achieve ultra high conductivity, but unfortunately is forced to give up porosity as a fabric. However, coaxial cladding structures are intended to apply rGO to the surface of each fiber, thus preserving the original structure, but limiting conductivity due to lack of continuity of the rGO network, which requires a corresponding solution.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber and the preparation method thereof, by the method, W-NPFs can be recovered and reused, the loose fiber network characteristics of the W-NPFs are kept, meanwhile, the NPFs are endowed with a functional layer coaxially coated by rGO, higher conductivity is provided, the conductivity and the number of functional groups can be regulated and controlled, and sites are provided for possible chemical modification.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of a polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber comprises the following steps:
(1) Firstly, stripping Graphene Oxide (GO) in a high-pressure homogenizer, and then dispersing the Graphene Oxide (GO) in water in an ultrasonic generator to obtain GO aqueous solution for later use;
(2) Placing the washed and abandoned non-woven polypropylene fabrics (W-NPFs) into a mixed solution of a swelling agent and a surfactant for treatment for a period of time, drying, and repeating the steps for a plurality of times to obtain modified non-woven polypropylene fabrics (T-NPFs);
(3) Soaking the T-NPFs prepared in the step (2) in the GO aqueous solution in the step (1), and then drying and repeating the soaking and drying steps for a plurality of times to obtain the polypropylene hydrocarbon/graphene oxide coaxial coated fibers (GO-NPFs);
(4) And (3) placing the GO-NPFs prepared in the step (3) in a reducing agent for treatment, and then cleaning and drying to obtain the polypropylene/graphene oxide coaxial coated high-conductivity fibers (rGO-NPFs).
Preferably, graphene Oxide (GO) in the step (1) is prepared by oxidizing graphite by a modified Hummers method, wherein the graphite is flake graphite, natural graphite or expanded graphite, and the diameter of a graphite sheet is 50nm to 3 mu m; the pressure of the high-pressure homogenizer is 120 Torr, and the dispersion time is 30min.
Preferably, the concentration of the aqueous GO solution in step (1) is from 0.1mg/ml to 10mg/ml.
Preferably, the washed waste nonwoven polypropylene fabrics (W-NPFs) in step (2) are obtained by sterilizing, washing and drying the recovered W-NPFs in 75% ethanol aqueous solution.
Preferably, in the step (2), the swelling agent is a mixed solution of ethyl acetate and water in a volume ratio of 1:1, and the treatment time is 36 hours.
Preferably, the surfactant in the step (2) is triton, and the amount of the surfactant is 0.5wt% of the swelling agent solution.
Preferably, the number of times of repeated soaking and drying steps in the step (4) is 1-16 times.
Preferably, in the step (4), the reducing agent is thiourea dioxide solution or sodium borohydride solution, and the mass concentration of the reducing agent is 0.5%.
Preferably, the preparation method of the improved hummers method graphene oxide comprises the following steps:
(1) Weighing 10g of graphene, pouring the graphene into a beaker, weighing 200ml of concentrated sulfuric acid, pouring the concentrated sulfuric acid into the beaker, putting the magnetic particles into the beaker, stirring the mixture for 2 hours by using a magnetic stirrer, and adding 30g of potassium permanganate during the stirring process, wherein the adding is completed for 1 hour; (2) putting the beaker into an ultrasonic cleaner for 8 hours; (3) Placing the beaker on a magnetic stirrer, slowly adding 450ml deionized water while stirring, and stirring for 1h; (4) Adding 1400ml deionized water, adding 150ml hydrogen peroxide, taking down the beaker and standing; (5) Pouring out the supernatant to obtain a base solution, and centrifuging the base solution by using a centrifugal machine until the pH value is 6; (6) Pouring the graphene oxide into a surface dish, and putting the surface dish into an oven for drying to obtain the graphene oxide.
In addition, the invention also claims the polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber prepared by the preparation method.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention carries out coaxial coating modification on the formed commercial product, thereby greatly reducing the cost and difficulty;
2. after being coated on a material for molding, the triton X-100 does not affect the physical and chemical properties of polypropylene;
3. the small-size graphene disclosed by the invention is not similar to the film forming on the whole surface of a material in the prior art, but is used for coaxially coating each fiber in the melt-blown fabric, so that the micro-nano structure and the characteristics of the melt-blown fabric are greatly reserved;
4. the chemical reagents are all safe and nontoxic products, and accord with the environmental protection concept.
Drawings
FIG. 1 is a sample graph of rGO-NPFs prepared in example 1 of this invention;
FIG. 2 is a surface Scanning Electron Microscope (SEM) of rGO-NPFs prepared in example 1 of this invention;
FIG. 3 is a Scanning Electron Microscope (SEM) of the coated rGO-NPFs prepared in example 1 of this invention;
FIG. 4 shows the conductivities of the samples obtained in examples 1-5 of the present invention.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
Example 1
A preparation method of a polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber comprises the following steps:
(1) Firstly screening crystalline flake graphite with equivalent sheet diameter smaller than 1.13 mu m by a 10000-mesh screen, then treating the screened crystalline flake graphite by an improved Hummers method to obtain Graphene Oxide (GO), repeatedly stripping the Graphene Oxide (GO) under the pressure of 120 Torr of a high-pressure homogenizer, and dispersing the Graphene Oxide (GO) in water for 30min in an ultrasonic generator to obtain GO aqueous solution with concentration of 1mg/ml for later use;
(2) Placing the recovered waste non-woven polypropylene fabrics (W-NPFs) in 75% ethanol water solution for disinfection, washing and drying to obtain washed waste non-woven polypropylene fabrics (W-NPFs), then placing the washed waste non-woven polypropylene fabrics (W-NPFs) in a mixed solution of ethyl acetate and water of triton X-100 for 24 hours, and then placing in an environment of 60 ℃ for drying to obtain modified non-woven polypropylene fabrics (T-NPFs); wherein the volume ratio of ethyl acetate to water is 1:1, and pull-through X-100 accounts for 0.5 percent of the mass of the mixed solution of ethyl acetate and water;
(3) Placing the T-NPFs prepared in the step (2) in the GO aqueous solution in the step (1) for infiltration treatment for 30min under micro-flow, taking out and drying, and repeating the infiltration and drying steps for 1 time to obtain the polypropylene/graphene oxide coaxial coated fibers (GO-NPFs);
(4) And (3) placing the GO-NPFs prepared in the step (3) into thiourea dioxide aqueous solution with the temperature of 60 ℃ and the concentration of 0.5mol/L for reduction for 30s, then kneading and washing under flowing water and drying at the temperature of 75 ℃ to obtain the polypropylene/graphene oxide coaxial-coated high-conductivity fibers (rGO-NPFs).
Example 2
A preparation method of a polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber comprises the following steps:
(1) Firstly screening crystalline flake graphite with equivalent sheet diameter smaller than 1.13 mu m by a 10000-mesh screen, then treating the screened crystalline flake graphite by an improved Hummers method to obtain Graphene Oxide (GO), repeatedly stripping the Graphene Oxide (GO) under the pressure of 120 Torr of a high-pressure homogenizer, and dispersing the Graphene Oxide (GO) in water for 30min in an ultrasonic generator to obtain GO aqueous solution with concentration of 1mg/ml for later use;
(2) Placing the recovered waste non-woven polypropylene fabrics (W-NPFs) in 75% ethanol water solution for disinfection, washing and drying to obtain washed waste non-woven polypropylene fabrics (W-NPFs), then placing the washed waste non-woven polypropylene fabrics (W-NPFs) in a mixed solution of ethyl acetate and water of triton X-100 for 24 hours, and then placing in an environment of 60 ℃ for drying to obtain modified non-woven polypropylene fabrics (T-NPFs); wherein the volume ratio of ethyl acetate to water is 1:1, and pull-through X-100 accounts for 0.5 percent of the mass of the mixed solution of ethyl acetate and water;
(3) Placing the T-NPFs prepared in the step (2) in the GO aqueous solution in the step (1) for infiltration treatment for 30min under micro-flow, taking out and drying, and repeating the infiltration and drying steps for 3 times to obtain the polypropylene/graphene oxide coaxial coated fibers (GO-NPFs);
(4) And (3) placing the GO-NPFs prepared in the step (3) into thiourea dioxide aqueous solution with the temperature of 60 ℃ and the concentration of 0.5mol/L for reduction for 30s, then kneading and washing under flowing water and drying at the temperature of 75 ℃ to obtain the polypropylene/graphene oxide coaxial-coated high-conductivity fibers (rGO-NPFs).
Example 3
A preparation method of a polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber comprises the following steps:
(1) Firstly screening crystalline flake graphite with equivalent sheet diameter smaller than 1.13 mu m by a 10000-mesh screen, then treating the screened crystalline flake graphite by an improved Hummers method to obtain Graphene Oxide (GO), repeatedly stripping the Graphene Oxide (GO) under the pressure of 120 Torr of a high-pressure homogenizer, and dispersing the Graphene Oxide (GO) in water for 30min in an ultrasonic generator to obtain GO aqueous solution with concentration of 1mg/ml for later use;
(2) Placing the recovered waste non-woven polypropylene fabrics (W-NPFs) in 75% ethanol water solution for disinfection, washing and drying to obtain washed waste non-woven polypropylene fabrics (W-NPFs), then placing the washed waste non-woven polypropylene fabrics (W-NPFs) in a mixed solution of ethyl acetate and water of triton X-100 for 24 hours, and then placing in an environment of 60 ℃ for drying to obtain modified non-woven polypropylene fabrics (T-NPFs); wherein the volume ratio of ethyl acetate to water is 1:1, and pull-through X-100 accounts for 0.5 percent of the mass of the mixed solution of ethyl acetate and water;
(3) Placing the T-NPFs prepared in the step (2) in the GO aqueous solution in the step (1) for infiltration treatment for 30min under micro-flow, taking out and drying, and repeating the infiltration and drying steps for 7 times to obtain the polypropylene/graphene oxide coaxial coated fibers (GO-NPFs);
(4) And (3) placing the GO-NPFs prepared in the step (3) into thiourea dioxide aqueous solution with the temperature of 60 ℃ and the concentration of 0.5mol/L for reduction for 30s, then kneading and washing under flowing water and drying at the temperature of 75 ℃ to obtain the polypropylene/graphene oxide coaxial-coated high-conductivity fibers (rGO-NPFs).
Example 4
A preparation method of a polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber comprises the following steps:
(1) Firstly screening crystalline flake graphite with equivalent sheet diameter smaller than 1.13 mu m by a 10000-mesh screen, then treating the screened crystalline flake graphite by an improved Hummers method to obtain Graphene Oxide (GO), repeatedly stripping the Graphene Oxide (GO) under the pressure of 120 Torr of a high-pressure homogenizer, and dispersing the Graphene Oxide (GO) in water for 30min in an ultrasonic generator to obtain GO aqueous solution with concentration of 1mg/ml for later use;
(2) Placing the recovered waste non-woven polypropylene fabrics (W-NPFs) in 75% ethanol water solution for disinfection, washing and drying to obtain washed waste non-woven polypropylene fabrics (W-NPFs), then placing the washed waste non-woven polypropylene fabrics (W-NPFs) in a mixed solution of ethyl acetate and water of triton X-100 for 24 hours, and then placing in an environment of 60 ℃ for drying to obtain modified non-woven polypropylene fabrics (T-NPFs); wherein the volume ratio of ethyl acetate to water is 1:1, and pull-through X-100 accounts for 0.5 percent of the mass of the mixed solution of ethyl acetate and water;
(3) Placing the T-NPFs prepared in the step (2) in the GO aqueous solution in the step (1) for infiltration treatment for 30min under micro-flow, taking out and drying, and repeating the infiltration and drying steps for 11 times to obtain the polypropylene/graphene oxide coaxial coated fibers (GO-NPFs);
(4) And (3) placing the GO-NPFs prepared in the step (3) into thiourea dioxide aqueous solution with the temperature of 60 ℃ and the concentration of 0.5mol/L for reduction for 30s, then kneading and washing under flowing water and drying at the temperature of 75 ℃ to obtain the polypropylene/graphene oxide coaxial-coated high-conductivity fibers (rGO-NPFs).
Example 5
A preparation method of a polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber comprises the following steps:
(1) Firstly screening crystalline flake graphite with equivalent sheet diameter smaller than 1.13 mu m by a 10000-mesh screen, then treating the screened crystalline flake graphite by an improved Hummers method to obtain Graphene Oxide (GO), repeatedly stripping the Graphene Oxide (GO) under the pressure of 120 Torr of a high-pressure homogenizer, and dispersing the Graphene Oxide (GO) in water for 30min in an ultrasonic generator to obtain GO aqueous solution with concentration of 1mg/ml for later use;
(2) Placing the recovered waste non-woven polypropylene fabrics (W-NPFs) in 75% ethanol water solution for disinfection, washing and drying to obtain washed waste non-woven polypropylene fabrics (W-NPFs), then placing the washed waste non-woven polypropylene fabrics (W-NPFs) in a mixed solution of ethyl acetate and water of triton X-100 for 24 hours, and then placing in an environment of 60 ℃ for drying to obtain modified non-woven polypropylene fabrics (T-NPFs); wherein the volume ratio of ethyl acetate to water is 1:1, and pull-through X-100 accounts for 0.5 percent of the mass of the mixed solution of ethyl acetate and water;
(3) Placing the T-NPFs prepared in the step (2) in the GO aqueous solution in the step (1) for infiltration treatment for 30min under micro-flow, taking out and drying, and repeating the infiltration and drying steps for 15 times to obtain the polypropylene/graphene oxide coaxial coated fibers (GO-NPFs);
(4) And (3) placing the GO-NPFs prepared in the step (3) into thiourea dioxide aqueous solution with the temperature of 60 ℃ and the concentration of 0.5mol/L for reduction for 30s, then kneading and washing under flowing water and drying at the temperature of 75 ℃ to obtain the polypropylene/graphene oxide coaxial-coated high-conductivity fibers (rGO-NPFs).
Performance testing was performed on the polypropylene/graphene oxide co-axially coated highly conductive fibers prepared in examples 1-5:
the conductivity detection method comprises the following steps: adopting a four-probe resistance tester to test, firstly cutting raw materials into raw sheets with the diameter of 5cm, secondly measuring, checking and recording the thickness of the sample, and ensuring that the thickness is not more than 400 microns; subsequently placing the four probes at a plurality of points greater than 1cm from the edge of the material for measurement; finally, the result is counted and an error bar is calculated, and the specific result is shown in fig. 4.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (5)
1. The preparation method of the polypropylene/reduced graphene oxide coaxial coated high-conductivity fiber is characterized by comprising the following steps of:
(1) Firstly, stripping Graphene Oxide (GO) in a high-pressure homogenizer, and then dispersing the Graphene Oxide (GO) in water in an ultrasonic generator to obtain GO aqueous solution for later use;
(2) Placing the washed and abandoned non-woven polypropylene fabrics (W-NPFs) into a mixed solution of a swelling agent and a surfactant for treatment for a period of time, drying, and repeating the steps for a plurality of times to obtain modified non-woven polypropylene fabrics (T-NPFs);
(3) Placing the T-NPFs prepared in the step (2) into the GO aqueous solution prepared in the step (1) for infiltration, and then drying and repeating the infiltration and drying steps for a plurality of times to obtain the polypropylene/graphene oxide coaxial coated fibers (GO-NPFs);
(4) The GO-NPFs prepared in the step (3) is placed in a reducing agent for treatment, and then is cleaned and dried, so that the polypropylene/reduced graphene oxide coaxial coated high-conductivity fibers (rGO-NPFs) are obtained;
the concentration of the GO aqueous solution in the step (1) is 0.1mg/ml to 10mg/ml;
the swelling agent in the step (2) is a mixed solution of ethyl acetate and water in a volume ratio of 1:1, and the treatment time is 36 hours;
the surfactant in the step (2) is triton, and the dosage of the surfactant is 0.5wt% of the swelling agent solution;
the reducing agent in the step (4) is thiourea dioxide solution or sodium borohydride solution, and the mass concentration of the reducing agent is 0.5%.
2. The preparation method according to claim 1, wherein the Graphene Oxide (GO) in the step (1) is prepared by oxidizing graphite by a modified Hummers method, the graphite is flake graphite, natural graphite or expanded graphite, and the diameter of the graphite flake is 50nm to 3 μm; the pressure of the high-pressure homogenizer is 120 Torr, and the dispersion time is 30min.
3. The method according to claim 1, wherein the washed waste nonwoven polypropylene fabrics (W-NPFs) in step (2) are obtained by sterilizing, washing and drying recovered W-NPFs in 75% aqueous ethanol.
4. The method according to claim 1, wherein the number of times of repeating the immersing and drying steps in the step (3) is 1 to 16.
5. A polypropylene/reduced graphene oxide coaxial-coated highly conductive fiber prepared by the preparation method of any one of claims 1 to 4.
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